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13C NMR spectra of 11α derivatives, and as a broad line or a triplet in the 11β-perfluoroalkylated spectra.
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The 9(11)-dehydro structure of 6 mainly relies on the presence of an isolated AB system for protons H12α and H12β (δ 2.31 and 2.35, respectively) identified by HCOR and DEPT (δ C12 = 40.8 ppm), and on the absence of coupling with other protons in a COSY experiment. The signals corresponding to these protons, although partially obscured, were more apparent in the debenzylated derivative 7 of 6 (δ 2.02 and 2.35 ppm, J = 14.6 Hz) and showed no further coupling.
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We greatly acknowledge one of the reviewers for this very interesting suggestion.
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